CN102610531A - Method for preparing diamond-silicon composite package material - Google Patents
Method for preparing diamond-silicon composite package material Download PDFInfo
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- CN102610531A CN102610531A CN2012100636253A CN201210063625A CN102610531A CN 102610531 A CN102610531 A CN 102610531A CN 2012100636253 A CN2012100636253 A CN 2012100636253A CN 201210063625 A CN201210063625 A CN 201210063625A CN 102610531 A CN102610531 A CN 102610531A
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Abstract
The invention relates to a method for preparing a diamond-silicon composite package material, which belongs to the field of electronic package materials. The method includes the steps: firstly, uniformly mixing diamond particles and silicon powder with the volume fraction of 40-70% with trace sintering aids including Al or Ti powder; secondly, placing a graphite mould containing mixture into an SPS (spark plasma sintering) device, pressurizing by 20-30MPa and vacuumizing; thirdly, rapidly sintering by the aid of inert gas or vacuum, setting holding temperature to range from 1250 DEG C to 1370 DEG C during sintering and setting sintering pressure to range from 40MPa to 60MPa; and fourthly, performing furnace cooling after sintering and depressurizing at the temperature lower than 1000 DEG C to obtain the compact composite material without microcracks. The method avoids the problems of diamond graphitization, silicon substrate oxidization and the like due to long sintering time. Various composite materials with different diamond contents can be obtained by changing the proportion of raw materials, and the method is high in operability and simple in process. The heat conductivity of the prepared composite material is as high as 515W/mK, the heat expansion rate of the prepared composite material is lower than 1.5X10-6/K, the compactness of the prepared composite material is higher than 99.6%, and the prepared composite material can be used for the fields of electronic package and the like.
Description
Technical field
The invention belongs to the Electronic Packaging field; Relate to a kind of diamond-novel preparation method of silicon composite encapsulating material, be specifically related to a kind of discharge plasma sintering and interpolation sintering aid of adopting and prepare the low diamond of density height, thermal conductivity height and thermal coefficient of expansion-silicon composite encapsulating material method.
Background technology
Along with hyundai electronics and fast development of information technology, also increasingly high to the heat dispersion requirement of basis material, research has combination property good electron encapsulating material and has a great deal of practical meanings.Improving constantly of chip integration, Electronic Packaging develops to miniaturization, lightweight and high performance direction, makes the working temperature of circuit constantly rise, and system unit volume heat generation rate constantly increases.In order to obtain stable performance, must improve radiating condition, Electronic Packaging constantly promotes in the importance of microelectronic, and the demand that is accompanied by the novel electron encapsulating material is also in continuous increase.
High quality diamond has the highest thermal conductivity and lower thermal coefficient of expansion, and thermal conductivity can reach 2000W/mK, and diamond has characteristics such as electric insulation, low-k in addition; Single diamond is difficult for being made into encapsulating material, and comparatively ideal is to be equipped with composite material with diamond particles as strengthening system.What at present research was more is that copper, aluminium, silver and silicon prepare diamond composite as basis material, wherein copper or silver as basis material have all that wetability is low, thermal coefficient of expansion and density is all than problems such as height; Aluminium gold diamond composite material thermal coefficient of expansion is too big, is difficult to use.The HIGH-PURITY SILICON material has lower density, high heat-conducting property and lower thermal coefficient of expansion, and density is 2.33g/cm
3, (thermal conductivity TC) is 160W/mK to thermal conductivity, and (coefficients of thermal expansion is 3.6 * 10 CTE) to thermal coefficient of expansion
-6/ K; Silicon and diamond wetability are good, generate carborundum at silicon and diamond interface place in the sintering process, have reduced interface resistance.Therefore, use significant for the research of diamond-silicon composite to this Development of Materials.
The problem of preparation diamond-silicon composite encapsulating material existence mainly comprises: (1) is difficult to adopt general preparation method to prepare fine and close diamond-silicon composite encapsulating material, adopts diamond-silicon composite density that nothing is pressed or HIP sintering prepares all very low.Can improve sintered density through in composite material, adding sintering aid, but density is still not high; (2) diamond graphitization very easily under hot conditions, the long diamond surface graphitization that makes of sintering time reduces composite property.
In recent years, only there is the pressure of employing infiltration method to prepare diamond-silicon composite.Adopt this method to prepare diamond/silicon composite; Because the vacuum degree that the preparation process need is high and the pressure of superelevation; High to equipment requirements, manufacturing cost and costliness thereof, largely limit the diamond/application of silicon composite electron encapsulating material in electronic engineering.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of diamond-silicon composite encapsulating material, this method prepared composite material interface contact is firm, and preparation technology is simple, and density and thermal property are significantly increased.
To achieve these goals, the technology side of the present invention's employing is: the preparation method of a kind of diamond-silicon composite encapsulating material is characterized in that this method comprises the steps:
(1) diamond particle, silica flour are evenly mixed with sintering aid, wherein, the volume fraction of silica flour is 40%～70%, and the volume fraction of sintering aid is 0～10%;
The graphite jig that (2) said mixture will be housed is put into the discharge plasma sintering stove, and pressurization 20～30MPa also vacuumizes;
(3) Fast Sintering, holding temperature is set at 1250～1370 ℃ during sintering, adopts inert gas or vacuum in the sintering process, and sintering pressure is 40～60MPa;
(4) sintering end back is carried out with the stove cooling to sample and is being laid down pressure below 1000 ℃, to obtain the fine and close composite material that does not have micro-crack.
As the improvement of technique scheme, in the step (3), the temperature retention time 3～5min in the sintering process, heating rate are 50～150 ℃/min.
As the further improvement of technique scheme, inert gas is an argon gas, and vacuum degree is less than 10Pa.
Said sintering aid is Al powder or Ti powder preferably.
(spark plasma sintering, SPS) Fast Sintering and powder metallurgic method combine, and through the control of composition and process, optimize technological parameter and improve the sample combination property with the discharge plasma sintering stove in the present invention.Silicon and diamond interface form the carborundum transition zone, have significantly reduced interface resistance; Add micro-sintering aid and effectively improve the sample density.Particularly, technique effect of the present invention is following:
1) diamond particles is evenly distributed, and and silicon substrate between interface cleaning firmly
Adopted SPS Fast Sintering method among the present invention, made in-situ chemical reaction generation carborundum transition zone takes place between diamond particle and the silica flour, improved the sample density through regulation and control then programming rate and temperature retention time.Add micro-sintering aid, help reducing sintering temperature and reduce sintering time; Selection sintering end back is carried out with the stove cooling to sample and is being laid down pressure below 1000 ℃, helps densified sintering product and reduces micro-crack.It is high behind process optimization, to make the example interface bonding strength, and no microscopic defect exists.
2) low, technology of synthesis temperature and equipment are simple, and combination property is good
The sintering maximum temperature is 1370 ℃ in this technology, and under vacuum (less than 10Pa) or argon gas atmosphere, heating rate is fast and temperature retention time short, can effectively stop the diamond graphitization in utmost point chien shih sample densification in short-term.Total building-up process has equipment and advantage such as technology is simple, synthesis temperature is low, and prepared composite material thermal conductivity is up to 515W/mK, and thermal expansion is lower than 1.5 * 10
-6/ K, density reaches more than 99.6%.
Capital equipment used in the present invention is: discharge plasma sintering stove (SPS).
3) optimize properties of product
Adopt Fast Sintering method and interpolation sintering aid to combine, can obtain the diamond that density is low, thermal conductivity is high and thermal coefficient of expansion is low-silicon composite encapsulating material.Wherein, can regulate the thermal conductivity and the thermal coefficient of expansion of material through the content of regulating diamond particle, along with the raising thermal conductivity of diamond content increases thereupon, thermal coefficient of expansion decreases; The high more composite material thermal conductivity that obtains of the grade of diamond particle is high more; Also can regulate material property through regulating the diamond particles size, but increase not obvious along with the diamond particle diameter increases thermal conductivity.
Description of drawings
Fig. 1 is the section SEM figure of sample, a) is instance 2 sample section figure wherein; B) be instance 1 sample section figure; C) be instance 5 sample section figure.
Fig. 2 is instance 2 sample surfaces, wherein a) for amplifying 20 times, b) for amplifying 300 times.
Fig. 3 is that instance 1 sample section line sweep can spectrogram, a) be sectional drawing wherein, b) for some A to a some B line ability spectrogram.
Fig. 4 is instance 2 a sample section line sweeps ability spectrogram, a) is sectional drawing, b) arrives a some B line ability spectrogram for some A.
Fig. 5 is instance 3 sample section SEM figure.
Fig. 6 is instance 4 sample section SEM figure.
Fig. 7 is that instance 5 sample section line sweeps can spectrogram, a) be sectional drawing wherein, b) for some A to a some B line ability spectrogram.
Fig. 8 is instance 6 sample section SEM figure.
Fig. 9 is that instance 5 sample section microcell EDS can spectrogram, a) be sectional drawing wherein, b) is black box microcell ability spectrogram.
Embodiment
The operation principle of the inventive method is: utilize the plasma discharging Fast Sintering; Make the silicon substrate particle under the silicon fusing point, in-situ chemical reaction take place in sintering process and diamond particles; Generate the interface silicon carbide layer, and the control of pressure obtains fine and close diamond-silicon composite when adding micro-sintering aid with cooling.
Condition and technology:
1) preparation condition and equipment
Sintering adopts discharge plasma sintering stove (SPS), and X-ray diffractometer (XRD) is adopted in the thing identification of phases, and microstructure observation adopts environment electron microscope (SEM with analysis; LEO 1450VP), L457 thermal constant tester is adopted in the thermal conductivity test, and thermal coefficient of expansion adopts NETZSCH DIL402PC.
2) selection of sintering process
Sintering temperature is 1250～1370 ℃, selects different sintering temperatures according to the different materials system, and is incubated 3～5min, makes sample carry out with the stove cooling subsequently and is laying down pressure below 1000 ℃, and concrete parameter is seen in each instance.
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with accompanying drawing and embodiment.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
Raw material used in the present invention is as shown in table 1:
Table 1
Wherein FDP type diamond is low article grade diamond, and MBD8 is a high grade diamond.
Instance 1:
Table 2 is selected material system and composition proportion:
Table 2 proportion of raw materials
With average grain diameter is that FDP type diadust and high-purity silicon powder about 100 μ m mixes; Mixed powder is in discharge plasma sintering furnace mould; Begin sintering once when vacuum degree reaches 10Pa, be heated to 1370 ℃ with 50 ℃/min of heating rate, temperature retention time is 3min; Sintering pressure is 30～60MPa, then with stove cooling and laying down pressure below 1000 ℃.Obtain diamond-silicon composite, its density is 2.96g/cm
3, thermal conductivity is 302W/mK, thermal coefficient of expansion is 1.627 * 10
-6/ K.
, the XRD material phase analysis comprises Diamond, three kinds of things of SiC and Si mutually in the sample after finding sintering; The sample densified sintering product, sample section (Fig. 1 (b)) does not all have hole; In conjunction with XRD material phase analysis and sample section line sweep (Fig. 3), silicon carbide layer at diamond and silicon at the interface.
Instance 2:
This instance adopts identical mixed material with instance 1; Mixed powder stops vacuum pump once when vacuum degree reaches 10Pa in discharge plasma sintering furnace mould, charge into argon gas; When gas pressure 0.03MPa for to be heated to 1370 ℃ with 50 ℃/min of heating rate; Temperature retention time is 3min, and sintering pressure is 30～60MPa, then with stove cooling and laying down pressure below 1000 ℃.Obtain diamond-silicon composite, its density is 2.97g/cm
3, thermal conductivity is 346W/mK, thermal coefficient of expansion is 1.553 * 10
-6/ K.
This sintered sample comprises Diamond, three kinds of things of SiC and Si mutually through the XRD material phase analysis; The sample densified sintering product, sample surfaces (Fig. 2) and section (Fig. 1 (a)) all do not have hole; In conjunction with XRD material phase analysis and sample section line sweep (Fig. 4), silicon carbide layer at diamond and silicon at the interface.
Different sintering conditions (vacuum, argon gas) sample microscopic structure and indistinction behind sintering, but the sample of sintering preparation has high thermal and lower thermal coefficient of expansion under the argon gas condition.
Instance 3:
Table 2 is selected material system and composition proportion:
Table 3 proportion of raw materials
With average grain diameter is that MBD8 type diadust and high-purity silicon powder about 100 μ m mixes, and mixed powder is in discharge plasma sintering furnace mould, and sintering process is identical with instance 2.Obtain diamond-silicon composite, its density is 2.972g/cm
3, thermal conductivity is 497W/mK, thermal coefficient of expansion is 1.517 * 10
-6/ K.
This sintered sample comprises Diamond, three kinds of things of SiC and Si mutually through the XRD material phase analysis; The sample densified sintering product, the no hole of sample section (Fig. 5);
Under the same terms, adopt different grade diamond particles, obtain the composite material thermal conductivity and significantly improve as strengthening body.
Instance 4:
This instance and instance 3 adopts identical proportioning raw materials, is that MBD8 type diadust and high-purity silicon powder about 300 μ m mixes with average grain diameter, and mixed powder is in discharge plasma sintering furnace mould, and sintering process is identical with instance 2.Obtain diamond-silicon composite, its density is 2.975g/cm
3, thermal conductivity is 515W/mK, thermal coefficient of expansion is 1.479 * 10
-6/ K.
This sintered sample comprises Diamond, three kinds of things of SiC and Si mutually through the XRD material phase analysis; The sample densified sintering product, the no hole of sample section (Fig. 6);
Under the same terms, the diamond particle that adopts different-grain diameter improves along with diamond particles increases the composite material thermal conductivity as strengthening body.
Instance 5:
The proportioning of table 4Diamond-Si
With average grain diameter is that FDP type diadust and high-purity silicon powder and micro-aluminium powder about 100 μ m mixes, and mixed powder is in discharge plasma sintering furnace mould, and sintering process is identical with instance 2.Obtain diamond-silicon composite, its density is 2.975g/cm
3, thermal conductivity is 264W/mK, thermal coefficient of expansion is 1.559 * 10
-6/ K.
This sintered sample comprises Diamond, SiC, four kinds of things of Al and Si mutually through the XRD material phase analysis; The sample densified sintering product, fracture apperance SEM figure (Fig. 1 (c)) and the EDS energy spectrum analysis (Fig. 7) of sample, the little metal Al that as can be seen from the figure adds mainly is distributed in silicon and at the interface adamantine.
Compare with instance 2, under the same process condition, the little metal Al of adding mainly is distributed in silicon and at the interface adamantine; Owing to add the fusing point that metallic aluminium has reduced silicon; Thereby reduced sintering temperature and improved sintered density, be liquid owing to aluminium under the hot conditions all dissolves, diffusion coefficient is bigger; Aluminium all is diffused into silicon and at the interface adamantine; But because the metallic aluminium that adds is going out with the interface with the second phase impurity form, thermal conductivity is had big inhibition, therefore add the corresponding reduction of thermal conductivity behind the metallic aluminium.
Instance 6:
The proportioning of table 4Diamond-Si
With average grain diameter is that MBD8 type diadust and high-purity silicon powder and micro-titanium valve about 100 μ m mixes, and mixed powder is in discharge plasma sintering furnace mould, and sintering process is identical with instance 2.Obtain diamond-silicon composite, its density is 2.99g/cm
3, thermal conductivity is 505W/mK, thermal coefficient of expansion is 1.459 * 10
-6/ K.
This sintered sample comprises Diamond, SiC, four kinds of things of TiSi2 and Si mutually through the XRD material phase analysis; The sample densified sintering product, fracture apperance SEM figure (Fig. 8) and the EDS energy spectrum analysis (seeing Fig. 9 (a), (b)) of sample; Wherein, among Fig. 9 (a), the component content in the little square frame film micro area is: Si; Mass fraction is 87.17Wt%, atomic fraction 92.05At%, Ti; Mass fraction is 12.83Wt%, atomic fraction 07.95At%.The main disperse of little metal Ti that as can be seen from the figure adds is distributed in the composite material.
Compare with instance 3, under the same process condition, the little metal Ti powder of adding has reduced the fusing point of silicon owing to add Titanium, has improved sintered density thereby reduced sintering temperature, therefore adds the corresponding raising of thermal conductivity behind the Titanium.
Instance 7:
The proportioning of table 5Diamond-Si
This instance reaches in vacuum degree and stops vacuum pump below the 10Pa; Charge into argon gas, for to be heated to 1250 ℃ with 150 ℃/min of heating rate, temperature retention time is 3min when gas pressure 0.03MPa; Sintering pressure is 30MPa, then with stove cooling and laying down pressure below 1000 ℃.Obtain diamond-silicon composite, its density is 2.78g/cm
3, thermal conductivity is 235W/mK, thermal coefficient of expansion is 2.079 * 10
-6/ K.
Instance 8:
The proportioning of table 4Diamond-Si
This instance reaches in vacuum degree and stops vacuum pump below the 10Pa; Charge into argon gas, for to be heated to 1250 ℃ with 150 ℃/min of heating rate, temperature retention time is 3min when gas pressure 0.03MPa; Sintering pressure is 30MPa, then with stove cooling and laying down pressure below 1000 ℃.Obtain diamond-silicon composite, its density is 2.6g/cm
3, thermal conductivity is 206W/mK, thermal coefficient of expansion is 2.153 * 10
-6/ K.
Those skilled in the art will readily understand; The above is merely preferred embodiment of the present invention; Not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, be equal to and replace and improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. the preparation method of diamond-silicon composite encapsulating material is characterized in that, this method comprises the steps:
(1) diamond particle, silica flour are evenly mixed with sintering aid, wherein, the volume fraction of silica flour is 40% ~ 70%, and the volume fraction of sintering aid is 0 ~ 10%;
The graphite jig that (2) said mixture will be housed is put into the discharge plasma sintering stove, and pressurization 20 ~ 30MPa also vacuumizes;
(3) Fast Sintering, holding temperature is set at 1250 ~ 1370 ℃ during sintering, adopts inert gas or vacuum in the sintering process, and sintering pressure is 40 ~ 60MPa;
(4) sintering end back is carried out with the stove cooling to sample and is being laid down pressure below 1000 ℃, to obtain the fine and close composite material that does not have micro-crack.
2. the preparation method of diamond according to claim 1-silicon composite encapsulating material is characterized in that: in the step (3), the temperature retention time 3 ~ 5min in the sintering process, heating rate are 50 ~ 150 ℃/min.
3. the preparation method of diamond according to claim 1 and 2-silicon composite encapsulating material is characterized in that: in the step (3), inert gas is an argon gas, and vacuum degree is less than 10Pa.
4. the preparation method of diamond according to claim 1 and 2-silicon composite encapsulating material is characterized in that: said sintering aid is Al powder or Ti powder.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107200586A (en) * | 2017-07-04 | 2017-09-26 | 北京理工大学 | A kind of TiB2The fast preparation method of ceramic block |
| CN111320476A (en) * | 2020-04-13 | 2020-06-23 | 北京科技大学广州新材料研究院 | Diamond-silicon carbide composite material, preparation method thereof and electronic equipment |
| CN111730054A (en) * | 2020-06-30 | 2020-10-02 | 湖南大学 | Low-temperature synthesis method and application of silicon carbide coated diamond composite powder |
| CN112142440A (en) * | 2020-09-15 | 2020-12-29 | 江汉大学 | Diamond film radiating fin and preparation method thereof |
| CN112625657A (en) * | 2019-09-24 | 2021-04-09 | 华为技术有限公司 | Packaging structure of heat conductor, heat conduction material and semiconductor device |
| CN112723902A (en) * | 2020-12-28 | 2021-04-30 | 华侨大学 | Slurry direct-writing forming method of diamond tool |
| CN114315354A (en) * | 2021-12-29 | 2022-04-12 | 武汉理工大学 | Diamond-B4Two-step sintering method of C-SiC three-phase composite ceramic |
| CN116393677A (en) * | 2023-04-07 | 2023-07-07 | 哈尔滨工业大学 | Method for preparing diamond/aluminum composite material by high-flux near-net forming |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107200586A (en) * | 2017-07-04 | 2017-09-26 | 北京理工大学 | A kind of TiB2The fast preparation method of ceramic block |
| CN107200586B (en) * | 2017-07-04 | 2020-08-07 | 北京理工大学 | TiB2Rapid preparation method of ceramic block |
| CN112625657A (en) * | 2019-09-24 | 2021-04-09 | 华为技术有限公司 | Packaging structure of heat conductor, heat conduction material and semiconductor device |
| CN111320476A (en) * | 2020-04-13 | 2020-06-23 | 北京科技大学广州新材料研究院 | Diamond-silicon carbide composite material, preparation method thereof and electronic equipment |
| CN111730054A (en) * | 2020-06-30 | 2020-10-02 | 湖南大学 | Low-temperature synthesis method and application of silicon carbide coated diamond composite powder |
| CN112142440A (en) * | 2020-09-15 | 2020-12-29 | 江汉大学 | Diamond film radiating fin and preparation method thereof |
| CN112723902A (en) * | 2020-12-28 | 2021-04-30 | 华侨大学 | Slurry direct-writing forming method of diamond tool |
| CN112723902B (en) * | 2020-12-28 | 2022-07-29 | 华侨大学 | Slurry direct-writing forming method of diamond tool |
| CN114315354A (en) * | 2021-12-29 | 2022-04-12 | 武汉理工大学 | Diamond-B4Two-step sintering method of C-SiC three-phase composite ceramic |
| CN116393677A (en) * | 2023-04-07 | 2023-07-07 | 哈尔滨工业大学 | Method for preparing diamond/aluminum composite material by high-flux near-net forming |
| CN116393677B (en) * | 2023-04-07 | 2023-11-03 | 哈尔滨工业大学 | Method for preparing diamond/aluminum composite material by high-flux near-net forming |
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Application publication date: 20120725 |